反应详情

4-Azido-7-cyanochroman (Step D) (4.3 g, 21 mmol) was dissolved in EtOAc (200 mL) and purged with N2. Pd/C (10%, 0.6 g) was added and the reaction was purged with N2. The reaction was purged with H2 and rapidly stirred under a H2 atmosphere until consumption of starting material was complete by TLC analysis (approximately 1 h). The reaction was purged with N2, and filtered through Celite®. The Celite®was washed with MeOH. The solution was concentrated in vacuo to provide a residue which was purified by column chromatography (silica, 3% MeOH in CH2Cl2 plus 0.5% NH4OH) to provide the title compound. TLC Rf=0.3 (5% MeOH in CH2Cl2 plus 0.5% Et3N.

1. custompurged with N2
2. additionPd/C (10%, 0.6 g) was added
3. customthe reaction was purged with N2
4. customThe reaction was purged with H2
5. customwas complete by TLC analysis (approximately 1 h)
6. customThe reaction was purged with N2
7. filtrationfiltered through Celite®
8. washThe Celite®was washed with MeOH
9. concentrationThe solution was concentrated in vacuo
10. customto provide a residue which
11. customwas purified by column chromatography (silica, 3% MeOH in CH2Cl2 plus 0.5% NH4OH)